Zirconium oxide dispersion and its preparation method and application

Abstract

The present invention discloses a zirconium oxide dispersion liquid and its preparation method and application, belonging to the technical field of zirconium oxide materials. The zirconium oxide dispersion liquid comprises a zirconium oxide component, a dispersant and a resin component; the pore volume of the zirconium oxide raw material used in the zirconium oxide component is ≤0.3cm 3 / g, and the pore size of the zirconium oxide raw material is ≤12nm. The preparation of the zirconium oxide dispersion comprises: mixing a mixed solution containing an organic solvent, a zirconium oxide component, and a dispersant with a resin component, and then removing the organic solvent. By preparing the zirconium oxide dispersion using the zirconium oxide raw material with the aforementioned pore volume and pore size, after the zirconium oxide dispersion is formed into a film, the resulting film can be subjected to a weathering test at a temperature of 85°C and a humidity of 85% for 240 hours, and the light attenuation can still be maintained below 2%, indicating good weathering stability and a long service life. The resulting film can be used to adjust the optical path.

Description

Technical Field

[0001] The present invention relates to the technical field of zirconium oxide materials, and in particular to a zirconium oxide dispersion liquid and a preparation method and application thereof. Background Art

[0002] Because nano-zirconia has the characteristics of high refractive index, light transmittance in the visible light region, good wear resistance and excellent corrosion resistance, it has been often used in recent years to be compounded with resin to prepare stable nano-dispersion liquid for use in various optical fields.

[0003] However, the film products prepared from zirconium oxide dispersion in the prior art have poor weather resistance, resulting in poor optical performance.

[0004] In view of this, the present invention is proposed. Summary of the Invention

[0005] The purpose of the present invention is to provide a zirconium oxide dispersion and a preparation method and application thereof, so as to solve or improve the above technical problems.

[0006] The present invention can be achieved like this:

[0007] In a first aspect, the present invention provides a zirconium oxide dispersion comprising a zirconium oxide component, a dispersant, and a resin component;

[0008] The pore volume of the zirconium oxide raw material used in the zirconium oxide component is ≤0.3cm 3 / g, and the pore size of the zirconium oxide raw material is ≤12nm.

[0009] In an optional embodiment, the average particle size of the zirconium oxide raw material is 1 nm to 50 nm.

[0010] In an optional embodiment, the average particle size of the zirconium oxide raw material is 5 nm to 20 nm.

[0011] In an optional embodiment, the content of the zirconium oxide raw material in the zirconium oxide dispersion is 40 wt % to 75 wt %.

[0012] In an optional embodiment, the content of the zirconium oxide raw material in the zirconium oxide dispersion is 45 wt % to 70 wt %.

[0013] In an optional embodiment, the content of the zirconium oxide raw material in the zirconium oxide dispersion is 50 wt % to 65 wt %.

[0014] In an optional embodiment, the amount of the dispersant used is 1 wt% to 20 wt% of the zirconium oxide raw material, preferably 5 wt% to 10 wt%.

[0015] In an optional embodiment, the zirconium oxide component is obtained by modifying a zirconium oxide raw material with a surface modifier.

[0016] In an optional embodiment, the amount of the surface modifier is 1 wt% to 30 wt% of the zirconium oxide raw material, preferably 5 wt% to 20 wt%;

[0017] In an optional embodiment, the surface modifier includes at least one of an organic acid compound, a phosphonic acid compound, a coupling agent, and a chelating agent.

[0018] In an optional embodiment, the coupling agent is a silane coupling agent, or the organic acid compound is an organic acid modifier containing a double bond.

[0019] In an alternative embodiment, the resin component is an optical resin.

[0020] In an optional embodiment, the resin component is a UV-curable acrylic resin.

[0021] In a second aspect, the present invention provides a method for preparing a zirconium oxide dispersion according to any one of the aforementioned embodiments, comprising the following steps: mixing a mixed solution containing an organic solvent, a zirconium oxide component, and a dispersant with a resin component, and then removing the organic solvent.

[0022] In an optional embodiment, the content of the zirconium oxide raw material in the mixed solution is 10 wt% to 80 wt%; preferably, the content of the zirconium oxide raw material in the mixed solution is 20 wt% to 50 wt%; more preferably, the content of the zirconium oxide raw material in the mixed solution is 20 wt% to 30 wt%.

[0023] In an optional embodiment, the organic solvent includes at least one of alcohols, ketones, ethers, esters, aliphatic hydrocarbons, cycloaliphatic hydrocarbons and aromatics; more preferably, the organic solvent includes at least one of propylene glycol methyl ether, propylene glycol methyl ether acetate, ethyl lactate, toluene, butanone and butyl acetate.

[0024] In a third aspect, the present invention provides a light path regulating coating, wherein the raw materials for preparing the light path regulating coating include the zirconium oxide dispersion of any one of the aforementioned embodiments.

[0025] In an optional embodiment, the raw materials for preparing the light path regulating coating further include an initiator.

[0026] In an optional embodiment, when the resin component is a UV-curable acrylic resin, the initiator is a photoinitiator.

[0027] In an optional embodiment, the amount of the photoinitiator is 1 wt% to 5 wt% of the zirconium oxide dispersion.

[0028] In a fourth aspect, the present invention provides a method for preparing a light path regulating coating as described in the aforementioned embodiment, comprising the following steps: coating the raw materials for preparing the light path regulating coating on the surface of a substrate, and curing the coating.

[0029] In an optional embodiment, the light transmittance of the substrate is not less than 89%, preferably not less than 90%.

[0030] In alternative embodiments, the substrate comprises polyethylene terephthalate, cellulose triacetate, polycarbonate, or polymethyl methacrylate.

[0031] In a fifth aspect, the present invention provides an application of a light path adjustment coating as described in the aforementioned embodiment, wherein the light path adjustment coating is used to adjust the light path.

[0032] In an optional embodiment, the light path regulating coating is used in LCD modules, lenses, cameras, architectural glass or optical adhesives.

[0033] The beneficial effects of the present invention include:

[0034] The present invention is achieved by using a pore volume of ≤0.3cm 3 / g of zirconium oxide raw material with a pore size of ≤12nm is used to prepare a zirconium oxide dispersion. After the zirconium oxide dispersion forms a film, the resulting film can be subjected to a weathering test at a temperature of 85°C and a humidity of 85% for 240 hours, and the light decay can still be maintained below 2%. It has good weathering stability and a long service life and is suitable for adjusting the optical path. If the pore volume and pore size of the zirconium oxide raw material are larger, on the one hand, the mass ratio of zirconium oxide at the same volume ratio after film formation will decrease. On the other hand, the larger the pore volume and pore size of the dispersion, the more likely it is to generate pores during the cross-linking and curing process. The combined effect of the above two aspects deteriorates the weathering resistance of the film after formation and reduces the optical efficacy of the film. DETAILED DESCRIPTION

[0035] To make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are described clearly and completely below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer are used. Where the manufacturer of the reagents or instruments is not specified, all are conventional products that can be purchased commercially.

[0036] The zirconium oxide dispersion provided by the present invention and its preparation method and application are described in detail below.

[0037] The present invention provides a zirconium oxide dispersion comprising a zirconium oxide component, a dispersant and a resin component.

[0038] The pore volume of the zirconium oxide raw material used in the zirconium oxide component is ≤0.3cm 3 / g, and the pore size of the zirconium oxide raw material is ≤12nm.

[0039] Zirconia dispersions prepared from zirconium oxide raw materials with different pore volumes and pore diameters have different weather resistance after film formation, and the impact is relatively large. The present invention creatively prepares a zirconium oxide dispersion using a zirconium oxide raw material with the above-mentioned pore volume and pore diameter. After the zirconium oxide dispersion is formed into a film, the obtained film can be subjected to a weathering test at a temperature of 85°C and a humidity of 85% for 240 hours, and the light decay can still be maintained below 2%, with good weathering stability and a long service life. It should be noted that the larger the pore volume and pore diameter of the zirconium oxide raw material, on the one hand, the lower the mass ratio of zirconium oxide at the same volume ratio after film formation, and on the other hand, the larger the pore volume and pore diameter of the dispersion during the cross-linking and curing process, the easier it is to generate pores; the above two aspects work together to worsen the weather resistance after film formation and reduce the optical efficacy of the film.

[0040] In some optional embodiments, the pore volume of the zirconium oxide raw material may be 0.0372 cm 3 / g, 0.0746cm 3 / g, 0.1163cm 3 / g, 0.1853cm 3 / g, 0.2012cm 3 / g, 0.2139cm 3 / g, 0.2427cm 3 / g, 0.2681cm 3 / g, 0.2801cm 3 / g or 0.2924cm 3 / g, etc., can also be ≤0.3cm 3 Other values ​​within the range of / g.

[0041] In some optional embodiments, the pore size of the zirconium oxide raw material can be 0.8645 nm, 1.1645 nm, 3.1145 nm, 5.4552 nm, 6.8235 nm, 8.2648 nm, 9.6626 nm, 10.0456 nm, 10.5896 nm or 11.7823 nm, or other values ​​within the range of ≤12 nm.

[0042] In some embodiments, the average particle size of the zirconium oxide raw material can be 1 nm to 50 nm, such as 1 nm, 5 nm, 10 nm, 15 nm, 20 nm, 25 nm, 30 nm, 35 nm, 40 nm, 45 nm, or 50 nm, or other values ​​within the range of 1 nm to 50 nm. In some preferred embodiments, the average particle size of the zirconium oxide raw material is 5 nm to 20 nm.

[0043] It should be noted that the present invention does not limit the crystal form of the zirconium oxide raw material. When used, zirconium oxide raw materials with monoclinic, tetragonal or mixed crystal forms can be used.

[0044] In the present invention, the content of the zirconium oxide raw material in the zirconium oxide dispersion can be 40 wt% to 75 wt%, such as 40 wt%, 45 wt%, 50 wt%, 55 wt%, 60 wt%, 65 wt%, 70 wt%, or 75 wt%, or other values ​​within the range of 40 wt% to 75 wt%. In some preferred embodiments, the content of the zirconium oxide raw material in the zirconium oxide dispersion is 45 wt% to 70 wt%. In some more preferred embodiments, the content of the zirconium oxide raw material in the zirconium oxide dispersion is 50 wt% to 65 wt%.

[0045] If the content of the zirconium oxide raw material in the zirconium oxide dispersion is lower than 40wt%, the refractive index of the prepared dispersion is low, which is not conducive to optical path adjustment; if the content of the zirconium oxide raw material in the zirconium oxide dispersion is higher than 75wt%, the dispersion cannot be prepared because the zirconium oxide content reaches the upper limit.

[0046] In the present invention, the zirconium oxide component is obtained by modifying the zirconium oxide raw material with a surface modifier.

[0047] By modifying the surface of the zirconium oxide raw material, the surface properties of the zirconium oxide raw material can be improved, and groups that are compatible with the resin can be grafted onto the surface of the zirconium oxide raw material.

[0048] The surface modification method is not limited, and can be, for example, grinding, heating, mixing and stirring.

[0049] The type of surface modifier is not limited, as long as it can play the role of affinity resin. In some embodiments, the surface modifier can include at least one of organic acid compounds with various types of groups, phosphonic acid compounds, coupling agents and chelating agents.

[0050] In some preferred embodiments, the surface modifier is at least one of a coupling agent and an organic acid modifier. Among them, the coupling agent is preferably a silane coupling agent, for example, a silane containing an acrylate group, a (meth) acrylic acid group, an epoxy group, an alkyl group, an alkoxy group, a vinyl group, a phenyl group, a methacryloxy group, an amino group, a chlorosilyl group, a chloropropyl group, or a mercapto group. The organic acid compound is preferably an organic acid modifier containing a double bond, for example, at least one of acrylic acid, methacrylic acid, ethyl acrylic acid, α-acrylic acid, β-methacrylic acid, α-phenyl acrylic acid, β-acryloyloxypropionic acid, sorbic acid, α-chlorosorbic acid, angelic acid, cinnamic acid, β-styryl acrylic acid, itaconic acid, maleic acid, citraconic acid, mesaconic acid, glutaconic acid, aconitic acid, and fumaric acid.

[0051] In some embodiments, the amount of the surface modifier can be 1 wt% to 30 wt% of the zirconia raw material, such as 1 wt%, 5 wt%, 10 wt%, 15 wt%, 20 wt%, 25 wt%, or 30 wt%, or other values ​​within the range of 1 wt% to 30 wt%. In some preferred embodiments, the amount of the surface modifier is 5 wt% to 20 wt% of the zirconia raw material.

[0052] In the present invention, the dispersant can assist in dispersing and wetting. The present invention does not impose any particular restrictions on the dispersing method; methods such as ultrasound, stirring, or grinding can be used. Furthermore, the present invention does not impose any restrictions on the type of dispersant; commercially available dispersants of various types and models can be used. Each dispersant can be used alone, or multiple dispersants can be combined for use.

[0053] In some optional embodiments, the dispersant may illustratively but not limitatively include at least one of BYK-P104, BYK-220S, BYK-110, BYK-111, BYK-170, BYK-171, BYK-180, BYK-181, BYK-174, BYK-2095, EFKA5010, EFKA5065, EFKA5066, EFKA5070, EFKA7500, EFKA7554, Solsperse3000, Sol-sperse16000, Sol-sperse17000, Sol-sperse18000, Sol-sperse36000, Sol-sperse36600 and Sol-sperse4100.

[0054] In some optional embodiments, the amount of the dispersant can be 1 wt% to 20 wt% of the zirconia raw material, such as 1 wt%, 2 wt%, 5 wt%, 8 wt%, 10 wt%, 12 wt%, 15 wt%, 18 wt%, or 20 wt%, or other values ​​within the range of 1 wt% to 20 wt%. In some preferred embodiments, the amount of the dispersant is 5 wt% to 10 wt% of the zirconia raw material.

[0055] In the present invention, the resin component is an optical resin. In some preferred embodiments, the resin component is a UV-curable acrylic resin, which can illustratively but not limitatively include at least one of benzyl acrylate, benzyl methacrylate, phenyl acrylate, diphenyl acrylate, phenoxybenzyl acrylate, 3-phenoxybenzyl acrylate, phenyl methacrylate, diphenyl methacrylate, 2-nitrophenyl acrylate, 4-nitrophenyl methacrylate, 2-nitrobenzyl methacrylate, 4-nitrobenzyl methacrylate, 2-chlorophenyl acrylate, 4-chlorophenyl acrylate, 2-chlorophenyl methacrylate, diphenylmethanol acrylate, 4-chlorophenyl methacrylate, o-phenylphenol ethyl acrylate, bisphenol diacrylate, hydroxyethyl acrylate, hydroxyethyl methacrylate, hexanediol diacrylate, tripropylene glycol diacrylate, ethylene glycol diacrylate, trimethylolpropane triacrylate, trimethylolpropane ethoxy triacrylate, glycerol propoxylated triacrylate, pentaerythritol tetraacrylate, and dipentaerythritol hexaacrylate.

[0056] In some embodiments, the amount of the resin can be obtained by subtracting the total content of the zirconium oxide raw material, the surface modifier, and the dispersant in the zirconium oxide dispersion from 100%.

[0057] Accordingly, the present invention also provides a method for preparing the above-mentioned zirconium oxide dispersion, which comprises the following steps: mixing a mixed solution containing an organic solvent, a zirconium oxide component and a dispersant with a resin component, and then removing the organic solvent.

[0058] In some embodiments, the zirconium oxide raw material is first modified with a surface modifier to obtain a zirconium oxide component; the zirconium oxide component is mixed with a dispersant and an organic solvent to obtain a mixed solution; the mixed solution is mixed with a resin component, and the organic solvent is removed to obtain a zirconium oxide dispersion.

[0059] In some embodiments, the content of the zirconium oxide raw material in the mixed solution may be 10 wt % to 80 wt %, such as 10 wt %, 20 wt %, 30 wt %, 40 wt %, 50 wt %, 60 wt %, 70 wt % or 80 wt %, or other values ​​within the range of 10 wt % to 80 wt %. In some preferred embodiments, the content of the zirconium oxide raw material in the mixed solution is 20 wt % to 50 wt %, and in some more preferred embodiments, the content of the zirconium oxide raw material in the mixed solution is 20 wt % to 30 wt %.

[0060] In some embodiments, the amount of the organic solvent can be obtained by subtracting the total content of the zirconium oxide raw material, the surface modifier, and the dispersant in the mixed solution from 100%.

[0061] The present invention does not specifically limit the organic solvent. In some embodiments, the organic solvent may include at least one of alcohols, ketones, ethers, esters, aliphatic hydrocarbons, cycloaliphatic hydrocarbons, and aromatics. In some preferred embodiments, the organic solvent may include at least one of propylene glycol methyl ether, propylene glycol methyl ether acetate, ethyl lactate, toluene, butanone, and butyl acetate.

[0062] The present invention does not impose any particular limitation on the method for removing the organic solvent. For example, but not limitation, a rotary evaporator or other vacuum distillation apparatus may be used for removal.

[0063] In addition, the present invention also provides a light path regulating coating, and the raw materials for preparing the light path regulating coating include the above-mentioned zirconium oxide dispersion.

[0064] Furthermore, the raw materials for preparing the optical path regulating coating also include an initiator.

[0065] In an optional embodiment, when the resin component is a UV-curable acrylic resin, the initiator is a photoinitiator.

[0066] The present invention is not particularly limited to photoinitiators. In some embodiments, the photoinitiator may include at least one of diazonium salt-based, sulfonium salt-based, and imidazole-based cationic photoinitiators. In other embodiments, the photoinitiator may also include at least one of free radical photoinitiators such as phosphorus-based, triazine-based, benzophenone-based, benzoin-based, oxime-based, acetone-based, aminoketone-based, ketone-based, anthraquinone-based, and aromatic phosphine oxide-based compounds. In some preferred embodiments, the photoinitiator may include at least one of TPO, 1173, 184, and 907.

[0067] In some embodiments, the amount of photoinitiator used can be 1wt% to 5wt% of the zirconium oxide dispersion, such as 1wt%, 1.5wt%, 2wt%, 2.5wt%, 3wt%, 3.5wt%, 4wt%, 4.5wt% or 5wt%, etc., or it can be other values ​​within the range of 1wt% to 5wt%.

[0068] Correspondingly, the present invention also provides a method for preparing the above-mentioned optical path regulating coating, comprising the following steps: coating the raw materials for preparing the optical path regulating coating on the surface of the substrate and curing.

[0069] The coating method is not particularly limited, and exemplary but not limiting methods include roller coating, spray coating, flow coating, or spin coating.

[0070] The coating substrate is also not particularly limited, and is preferably a substrate having a high transmittance. In some embodiments, the light transmittance of the substrate is not less than 89%, preferably not less than 90%. In some specific embodiments, the substrate may include polyethylene terephthalate, cellulose triacetate, polycarbonate, or polymethyl methacrylate.

[0071] The curing method can be achieved by using a mercury lamp, an LED, and the like, for example but not limited thereto.

[0072] In addition, the present invention also provides an application of the above-mentioned light path adjustment coating, which can be used to adjust the light path.

[0073] In some embodiments, the light path regulating coating can be used in LCD modules, lenses, cameras, architectural glass, or optical adhesives.

[0074] The features and performance of the present invention are further described in detail below with reference to the embodiments.

[0075] Example 1

[0076] The present invention provides a light path regulating coating, the preparation method of which comprises:

[0077] Step 1: Use 5g of silane coupling agent 3-(methacryloyloxy)propyltrimethoxysilane to 50g of zirconium oxide raw material powder (pore volume: 0.0372cm 3 After modification (with a pore size of 0.8645 nm and an average particle size of 10 nm), the modified zirconium oxide was obtained. The modified zirconium oxide was dispersed by ball milling in propylene glycol methyl ether (an organic solvent) using 2.5 g of BYK-110 dispersant to obtain a mixed solution. The raw zirconium oxide powder content in the mixed solution was 30 wt%.

[0078] Step 2: 42.5 g of 3-phenylbenzyl acrylate was added to the above mixed solution as a resin component, and propylene glycol methyl ether was removed by a rotary evaporator to obtain a zirconium oxide dispersion.

[0079] Step 3: Add 2 wt% of the photoinitiator TPO to the above zirconium oxide dispersion, and then apply it on PET to form a film by photocuring to obtain a light path regulating coating.

[0080] Example 2

[0081] The difference between this embodiment and embodiment 1 is that the pore volume of the zirconium oxide raw material powder is 0.0746 cm 3 / g, and the pore size is 1.1645nm.

[0082] Example 3

[0083] The difference between this embodiment and embodiment 1 is that the pore volume of the zirconium oxide raw material powder is 0.1163 cm 3 / g, pore size 3.1145nm. BYK-180 is the dispersant. Benzyl acrylate is the resin component. The amount of TPO photoinitiator used is 3wt% of the zirconium oxide dispersion.

[0084] Example 4

[0085] The difference between this embodiment and embodiment 1 is that the pore volume of the zirconium oxide raw material powder is 0.1853 cm 3 / g, with a pore size of 5.4552 nm. The dispersant is BYK-111. The resin component is diphenylmethanol acrylate. The amount of photoinitiator TPO used is 3 wt% of the zirconium oxide dispersion.

[0086] Example 5

[0087] The difference between this embodiment and embodiment 1 is that the pore volume of the zirconium oxide raw material powder is 0.2012 cm 3 / g, with a pore size of 6.8235nm. The silane coupling agent is γ-(2,3-epoxypropoxy)propyltrimethoxysilane. The content of zirconium oxide raw material powder in the mixed solution is 40wt%. The amount of resin component used is 25.8g. The amount of photoinitiator TPO used is 3wt% of the zirconium oxide dispersion.

[0088] Example 6

[0089] The difference between this embodiment and embodiment 5 is that the pore volume of the zirconium oxide raw material powder is 0.2139 cm 3 / g, pore size is 8.2648nm. The amount of resin component used is 19g.

[0090] Example 7

[0091] The difference between this embodiment and embodiment 6 is that the pore volume of the zirconium oxide raw material powder is 0.2427 cm 3 / g, and the pore size is 9.6626nm.

[0092] Example 8

[0093] The difference between this embodiment and embodiment 5 is that the pore volume of the zirconium oxide raw material powder is 0.2681 cm 3 / g, and the pore size is 10.0456nm.

[0094] Example 9

[0095] The difference between this embodiment and embodiment 5 is that the pore volume of the zirconium oxide raw material powder is 0.2801cm 3 / g, pore size is 10.5896nm. The amount of resin component used is 19g.

[0096] Example 10

[0097] The difference between this embodiment and embodiment 5 is that the pore volume of the zirconium oxide raw material powder is 0.2924 cm 3 / g, and the pore size is 11.7823nm.

[0098] Comparative Example 1

[0099] The difference between this comparative example and Example 1 is that the pore volume of the zirconium oxide raw material powder is 0.3111cm 3 / g, and the pore size is 12.5326nm.

[0100] Comparative Example 2

[0101] The difference between this comparative example and Example 2 is that the pore volume of the zirconium oxide raw material powder is 0.3526 cm 3 / g, and the pore size is 12.8252nm.

[0102] Comparative Example 3

[0103] The difference between this comparative example and Example 3 is that the pore volume of the zirconium oxide raw material powder is 0.3889 cm 3 / g, and the pore size is 13.7567nm.

[0104] Comparative Example 4

[0105] The difference between this comparative example and Example 4 is that the pore volume of the zirconium oxide raw material powder is 0.4270 cm 3 / g, and the pore size is 14.2333nm.

[0106] Comparative Example 5

[0107] The difference between this comparative example and Example 5 is that the pore volume of the zirconium oxide raw material powder is 0.4611cm 3 / g, and the pore size is 14.8749nm.

[0108] Comparative Example 6

[0109] The difference between this comparative example and Example 6 is that the pore volume of the zirconium oxide raw material powder is 0.4985 cm 3 / g, and the pore size is 15.5744nm.

[0110] Comparative Example 7

[0111] The difference between this comparative example and Example 7 is that the pore volume of the zirconium oxide raw material powder is 0.5331 cm 3 / g, and the pore size is 16.2365nm.

[0112] Comparative Example 8

[0113] The difference between this comparative example and Example 1 is that the pore volume of the zirconium oxide raw material powder is 0.2872 cm 3 / g, and the pore size is 13.5231nm.

[0114] Comparative Example 9

[0115] The difference between this comparative example and Example 1 is that the pore volume of the zirconium oxide raw material powder is 0.3472 cm 3 / g, and the pore size is 11.0645nm.

[0116] Comparative Example 10

[0117] This comparative example provides a preparation process in which the zirconium oxide content in the system is 76 wt %. The results show that a zirconium oxide dispersion cannot be obtained at this content.

[0118] The specific preparation steps include:

[0119] Step 1: Use 5g of silane coupling agent 3-(methacryloyloxy)propyltrimethoxysilane to 50g of zirconium oxide raw material powder (pore volume: 0.0372cm 3 After modification (with a pore size of 0.8645 nm and an average particle size of 10 nm), the modified zirconium oxide was obtained. The modified zirconium oxide was dispersed by ball milling in propylene glycol methyl ether (an organic solvent) using 2.5 g of BYK-110 dispersant to obtain a mixed solution. The raw zirconium oxide powder content in the mixed solution was 30 wt%.

[0120] Step 2: 8.29 g of 3-phenylbenzyl acrylate was added to the above mixed solution as a resin component. After removing propylene glycol methyl ether using a rotary evaporator, no zirconium oxide dispersion was obtained (the zirconium oxide content in the system was 76 wt %).

[0121] Test example

[0122] The light path regulating coatings prepared in Examples 1 to 10 and Comparative Examples 1 to 9 were subjected to weathering tests for 240 hours at a temperature of 85° C. and a humidity of 85%. The light attenuation of the films was then tested. The results are shown in Table 1.

[0123] Table 1 Test results

[0124]

[0125] As can be seen from Table 1, the optical path regulating coatings prepared in Examples 1 to 10 have better weathering stability than the optical path regulating coatings prepared in Comparative Examples 1 to 10, and the light attenuation can be kept below 2% after a weathering test for 240 hours under conditions of a temperature of 85°C and a humidity of 85%.

[0126] In summary, the present invention adopts a pore volume of ≤0.3cm3 A zirconium oxide dispersion prepared from zirconium oxide raw material with a pore size of ≤12nm can maintain light attenuation below 2% after 240 hours of weathering testing at 85°C and 85% humidity, demonstrating excellent weathering stability and a long service life. The resulting film can be used to adjust optical paths, such as in LCD modules, lenses, cameras, architectural glass, or optical adhesives.

[0127] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Those skilled in the art will readily appreciate that various modifications and variations of the present invention are possible. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.

Claims

1. Application of a zirconium oxide dispersion in the field of optics, characterized in that: The zirconium oxide dispersion comprises a zirconium oxide component, a dispersant and a resin component; The pore volume of the zirconium oxide raw material used in the zirconium oxide component is ≤0.3cm 3 / g, and the pore size of the zirconium oxide raw material is ≤12nm.

2. The use according to claim 1, characterized in that The average particle size of the zirconium oxide raw material is 1 nm to 50 nm.

3. The use according to claim 2, characterized in that The average particle size of the zirconium oxide raw material is 5nm~20nm.

4. The use according to claim 1, characterized in that The content of the zirconium oxide raw material in the zirconium oxide dispersion is 40 wt % to 75 wt %.

5. The use according to claim 4, characterized in that The content of the zirconium oxide raw material in the zirconium oxide dispersion is 45 wt % to 70 wt %.

6. The use according to claim 5, characterized in that The content of the zirconium oxide raw material in the zirconium oxide dispersion is 50 wt % to 65 wt %.

7. The use according to any one of claims 1 to 6, characterized in that The zirconium oxide component is obtained by modifying the zirconium oxide raw material with a surface modifier.

8. The use according to claim 7, characterized in that The amount of the surface modifier is 1 wt% to 30 wt% of the zirconium oxide raw material.

9. The use according to claim 8, characterized in that The amount of the surface modifier is 5 wt% to 20 wt% of the zirconium oxide raw material.

10. The use according to claim 7, characterized in that The surface modifier includes at least one of an organic acid compound, a coupling agent and a chelating agent.

11. The use according to claim 10, characterized in that The organic acid compounds include phosphonic acid compounds.

12. The use according to claim 10, characterized in that The coupling agent is a silane coupling agent, or the organic acid compound is an organic acid modifier containing a double bond.

13. The use according to any one of claims 1 to 6, characterized in that: The amount of the dispersant used is 1 wt% to 20 wt% of the zirconium oxide raw material.

14. The use according to claim 13, characterized in that The amount of the dispersant used is 5wt% to 10wt% of the zirconium oxide raw material.

15. The use according to any one of claims 1 to 6, characterized in that: The resin component is an optical resin.

16. The use according to claim 15, characterized in that The resin component is an ultraviolet light curing acrylic resin.

17. The use according to claim 1, characterized in that The method for preparing the zirconium oxide dispersion comprises the following steps: mixing a mixed solution containing an organic solvent, a zirconium oxide component and a dispersant with a resin component, and then removing the organic solvent.

18. The use according to claim 17, characterized in that The content of the zirconium oxide raw material in the mixed solution is 10 wt % to 80 wt %.

19. The use according to claim 18, characterized in that The content of the zirconium oxide raw material in the mixed solution is 20 wt % to 50 wt %.

20. The use according to claim 19, characterized in that The content of the zirconium oxide raw material in the mixed solution is 20 wt % to 30 wt %.

21. The use according to claim 17, characterized in that The organic solvent includes at least one of alcohols, ketones, ethers, esters, aliphatic hydrocarbons and aromatics.

22. The use according to claim 21, characterized in that The aliphatic hydrocarbons include cycloaliphatic hydrocarbons.

23. The use according to claim 21, characterized in that The organic solvent includes at least one of propylene glycol methyl ether, propylene glycol methyl ether acetate, ethyl lactate, toluene, butanone and butyl acetate.

24. A light path adjustment coating, characterized in that: The raw materials for preparing the optical path adjustment coating include the zirconium oxide dispersion used in any one of claims 1 to 16.

25. The optical path regulating coating according to claim 24, characterized in that: The raw materials for preparing the light path regulating coating also include an initiator.

26. The optical path regulating coating according to claim 25, characterized in that: When the resin component is an ultraviolet-curable acrylic resin, the initiator is a photoinitiator.

27. The optical path regulating coating according to claim 26, characterized in that: The amount of the photoinitiator used is 1 wt% to 5 wt% of the zirconium oxide dispersion.

28. A method for preparing the optical path regulating coating according to any one of claims 24 to 27, characterized in that: The following steps are involved: The raw materials for preparing the light path regulating coating are applied to the surface of the substrate and cured.

29. The preparation method according to claim 28, characterized in that The light transmittance of the substrate is not less than 89%.

30. The preparation method according to claim 29, characterized in that The light transmittance of the substrate is not less than 90%.

31. The preparation method according to claim 28, characterized in that The substrate includes polyethylene terephthalate, cellulose triacetate, polycarbonate or polymethyl methacrylate.

32. A use of the optical path regulating coating according to any one of claims 24 to 27, characterized in that: The light path adjustment coating is used to adjust the light path.

33. The use according to claim 32, characterized in that The light path regulating coating is used in LCD modules, lenses, cameras, architectural glass or optical adhesives.

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